The self-assembly of lignin (molecular and supramolecular) is driven mainly by non-covalent interactions, and the nature of the solvents and antisolvents directly affect the driving forces. The lignin particle is usually formed by noncovalently bonded cylindrical subunits. In this paper, we report a simple method which can be used to synthesize lignin nanoparticles by using spray freezing. The method is based on two properties of dimethyl sulfoxide (DMSO) that are excellent lignin solubility and a high melting point. Based on these two properties, kraft lignin solution in DMSO was sprayed onto liquid nitrogen-cooled copper plates using a handheld spray. The high melting point of DMSO caused immediate freezing and particle formation. The obtained particles were characterized for their size and morphology using dynamic light scattering (DLS), as well as scanning electron microscopy (SEM). Nano-range polydispersed particles were obtained by spraying 0.05% of lignin onto DMSO. This method can avoid lignin–solvent–antisolvent interactions, and can also be used to study lignin–lignin (subunits) and lignin–DMSO interactions.
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